Coffee concentrate and process of producing same



Sept. `23, 1958 L. NUTTING 2,853,337

COFFEE CONCENTRATE AND PROCESS OF' PRODUCING SAME Filed July 14, 1951 4 Sheets-Sheet 1 TEL? H Myrna.

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IN V EN TOR.

Sept. 23, 1958 L. NUTTING COFFEE CONCENTRATE AND PROCESS OF PRODUCING SAME Filed July 14, 1951 4 Sheets-Sheet 2 Sept. 23, 1958 L. NUTTING coFFFF CONCFNTRATF AND PRocFss 0F PRODUCING SAME Filed July 14, 19511 DE r 0 v Wm E? e m a nf. f n Nl R u Rw w w-r,. y w 1X n W M0 Enf D F 5 .i T M f m w s .n N. L. u T R w T i q R wp m vn ma man M m 4n. J M a i M 5B E HN H W M .a C

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IN V EN TOR.

HTTO HEYS Sept. 23, 1958 COFFEE CONCENTRATE AND PROCESS OF PRODUCING SAME 4 Sheets-Sheet 4 L. NUTTlNG COFFEE CONCENTRATE AND PROCESS F PRODUCING SAME Lee Notting, Berkeley, Calif., assgnor to Hills Bros. Cof# fee, Inc., San Francisco, Calif., a corporation of California Application July 14, 1951, serial No. 236,713

9 claims. (cl. 99-71) This invention relates to coffee concentrates and to the process of producing the same. This invention deals with the volatile flavoring matters ofcoee, the body material of the coffee extraction, and to the production of a new llavoring matter concentrate.

In my copending application, Serial No. 749,049, en-

? titled Process of Preparing a Coffee Concentrate, filed small in quantity, but are unstable in the presence of y waterl as separated. To prepare a satisfactory concentrate it is desirable to beable to adjustthe relationship of body material-to volatile flavoring matter'tomeet the conditions `of taste and use `to correspond with ,the flavor desires of different parties and sectionsof the consuming public. It is also desirable that such relationship be made adjustable so that a standard product may beproducedfrom varying roasts and blends of coffee to meet such davor requirements as exist.

It is therefore the object of my inventiontirst to provide a method of separating volatile liavoring matter fromr 2,853,387 Patented Sept. 23, 1958 ice the coffee are so processed as to reduce the liability of flavor loss both through the handling of the volatile con- 4 densate and through the volatilization of water both from I great damage.

, in the presence of water has little stability and is subject to rapid deterioration and loss.

fresh roasted ground coffee so as to obtain the maximum Of such volatile avors and second to provide a new volatile avoring concentrate, which is relatively stable and applicable for use for combining with a separately separated body material so as to produce either a stand ard ilavor value concentrater or a variation in the relation ship of the body material and the avoring valuesof the or process of stabilizing the volatile avoring matters extracted from roasted ground coffee. i A A Another object of my invention is to provide a method of producing a full flavored coffee concentrate wherein the composition of the coffee concentrate is controlledA to produce` a coffee brew havingva determined pH' value;

' Another object of this application is to set forth'and describe fully a series of variable processesand products which may be produced in accordance with my invention so that those skilled in the art will be ableto adjust the .process carried out vto meet the particulary desires and re-` quirements Aof the desired concentrateto be produced,

Another object of this invention is to provide -a series of processes of producing full flavored coffee concentrates of `dry form in each of which processes or methods the volatile' constituents obtained from lthe wet steaming'of the condensate and through the processing of the body material and condensate to produce the relatively dry coffee concentrate powder.

The processes of my invention are diagrammatically illustrated in the accompanying drawings in which Figure 1 isa diagrammatic flow sheet of a process embodying my invention.

`Figure 2 is a second diagrammatic flow sheet of the modified form of the process embodying my invention.

Figure 3 is a third diagrammatic flow sheet of a further modified form of process embodying my invention.

Figure 4 is a fourth diagrammatic ow sheet' of a further modified form of the process embodying my invention.

I have discovered several essentials to the production vof a full flavored powdered colfee concentrate which have enabled me to produce a full flavored coffee concentrate and have enabled me to maintain a variable in the process of production while retaining such full flavored value of .the ultimate product, all of which I believe will be apparent in the hereinafter set forth description of my invention through its several modifications as the same are illustrated in the accompanying ow sheets.

As coffee is processed in accordance with my copending application, Serial No. 749,049, the freshly roasted lground coffee is processed to produce two separated fractions, these being the volatile avoring matters and the body material. The body material is rather stable and may be subjected to rather strenuous processing without The volatile flavoring material separated When the economies of carrying out the process are -correct and the balance between body and flavoring matter in the freshly roasted coffee is precise, the process of my copending application may be followed with the production of a very satisfactory powdered coffee concentrate. When, however, it is desired or necessary for any reason to adjust the relationship between body material and volatile avoring matters in the ultimate dry concentrate, there is no way bywhich such adjustment can be satisfactorily made in accordance with the disclosure of my' aforesaid copending application. f

In a large scale application of my copending application if it is desired to adjust the relationship of body material to volatile flavoring matters, or it would be for any reason necessary to carry overfthe processing due to a lapse of time l'n operations, there is no way in which such a process could be carried out without loss of either oneof the two products produced, principally the volatile ground coffee is separated into a avor and a body mateflavoring matters. I have therefore discovered a method by which I am able to stabilize the volatile avoring matters in order to enable the relationship of the, two

.trate having stability which may be retained in anhydrous form or may be retained in anhydrous neutralized form so that it may be subsequently incorporated in the body material under such conditions as may be deemed ideal for carrying out the particular process of concentrates required.

Referring first to the process of Figure 1, the roasted rial portion in precisely the manner set forth in my costeam is then condensed to form a di'still'atejoffs't in fartd,A

'Safes 'volatile flavoring matters. The amount offc so collected is determinate of certain variables ",of''the process. It is of course preferable'that thesteain distillation be caried on for a period of time necessary to extract all the vo-latile liavoring' materials, including such g volatile acid constituents as may be separated bythis steam process.

The steam"'extractedcoffee' 'grounds are' then treated with hot water in such'manner as to' steep, percolate, or otherwise separate' from the ground roasted coffee those materials which are 'either water'soluble or Walter dispersible to produce an aqueous extraction of the body materials. This process is carried out in such manner as to utilize a` minimum of water consistent with the economics of the process in separating the body materials from the' ground roasted co-iiee.

In accordance Vwith my copending application above referred to, the aqueous extraction isthen concentrated, preferably by vacuum evaporation, to a point where the solid contents of the aqueous extraction are suciently high to enable the'reintroduction of the'steam distillate so that .upon subsequent drying of the mixed fractions, little flavoring value is lost.H There'is thus produced a dry cotfeeconcentrate of full flavoringfvalue.' By` dry as used inthisl' application; I do not meanfdry in the l chemical sense, 'but "merely a powder which has the ap pearance to theeye 'of being substantially dry.

This process is satisfactory where there is a maintainable and Adesired' balance between body material of the ground roasted coffee and thevolatile avoring matter extracted therefrom. It is also satisfactoryv where `no condition of operation is reached requiring'thef'discontinuance of the process where the steam distillate would be required to be retained for a period of time before reincorporation with the body material.

In accordance withthe 'present'invention Irthenproceed prior to reincorporation of the steam distillate 'with the body material to stabilize the 'steam distillate so'that Yits time or Vmanner'orreincorporation"with the vbody'rna terial may besuch as'good judgment dictates. Thus the steam distillate, in accordance with the process 'of Figure l, is extracted with ethyl ether which'hasgbee'n previously distilled'to remove all non-volatile impurities therefrom whichmight remain in the zseparated flavoring matters of thesteamdistillation.

The solvent which'I have herein set f orth is ethyl ether which is purified by distillation to'remove there-- from all constituents whichfrnig'ht remain in the flavoring matter of the vcoffee concentrate. Any'other suitable solvent free of non-volatile impurities may be'utilized such, for example, as propyl ether.

The adding of the ethyl ether to vtliesteam distillate 'y results in the avoring matters being dissolved'in ytheerthyl ether so that I am able to make a physical'separatiohj'of the water and ether containing the flavoring matters lby any suitable process well known to the'art such as 'by decantation. I then have anether extract which', how-v ever, carries with it some'gwater. It Ais then vfound d'e-A sirable in order that the flavoring matters have the highest stability, to' remove the waterfwhich is carriedover with the ether extract of the volatile'llavoring materials. To accomplish this I may utilize any suitable anhydrous medium such, for example, as anhydrousjso'diurn sulphate, which is added to the vether extract to` dehy'dratenfthe same and the resultant*sodiumvsulphate isremovedf'from the ether extract byltration'. 4I have thuspr'oduced an 'anhydrous ether yextract of the steam 'distillation of volatile avoring which shows a deterioration rate over a period of hours as compared with the steam distillate of tiavoring matter which has a deterioration rate measurable in minutes.

5 The anhydrous ether extract may then be reincorporated in the body material .to produce the dry coffee concentrate powder in anyV suitable manner. As illustrated i111thei1'owV sheet of Figure 1, the bodyv material aqueous extraction may be first'va'etuu'nY concentrated to the desired pointof solid content and then spray dried to produ'cefa' dry p'owderlf f This dry powder is then mixed/with A"the anhydrous' ether extract'to produce a slurry of the body material and volatile materials of the coffee, the ether in this casese'rving as a medium of dispersing the volatile avoring matters l,throughout the body material. After forming the slurry the'e'ther is" 'then distilled away so that it may be recovered for future use, leaving the dry coffee concentrate with restored flavor values.

' 'f The water containing concentrate of the body material has a relatively high ionic strength so that the'same does :not mix readily'with` thev ether solution of volatiles. It is 'l for this reason that the process as above set forth is suggested for. incorporating the anhydrous ether extract by fi'forming a` slurry with the dry body material. lAs differ- `entiating Yfrom the process of my copending application, v' this process does not reincorporate the volatile avoring matters into the body materials in such manner as to enablef'the body materials to exercise their greatest pro- "'tective'ability, over the volatile flavoring matters.

In accordance'with the process of Figure 2, precisely L" thesarneprocss is followed with the addition ofthe urtiier*stepy of neutralizing"thejystearn distillate'withka "siiitable'ag'entsuch, for example, as sodium bicarbonate to neutralize the acid contentof the steam distillate prior to ether'xtraction. Inv this step it is also found that by fthe laddition of a quantity of suitable salt with the sodium "bicarbonate vthat the neutral salts formed bythe reaction "ofthe-"sodium" bicarbonate with the acid of the `steam dis- 4Vtillate'are 'more'r'eadily separable from the ether soluble 40avorponstituents By neutralization as above set forth,

' I mean adjusting the pH of the steam distillate to a con- "f'dition inwhich the same has a pH value of approximately 6'.` In `this:neutr'ali'zation"step care should bel takento avoid raising the pH value beyond neutrality,lorof'a pH ".value of 7, asI have found'that to Vcai-"ry the saine beyond this point produces an" apparently irrevocable -flavor de "struction v v The-"steam distillate with the adjusted pH isthen Aex- A*tracted'with ethyl ether and dehydratedwith anhydrous `lfsodium*sulphate substantially as set forth in the process 'of'Figure 1. vIn thiscase there is produced an'anhy- "drous'f'ether extraction of the distillate with the pH ad- 'jsted' towardneutrality. vThis ether extract so produced is substantially free from volatile acids and has a deterioration rate measurable in days compared with th'less "stable ether extract of vvolatile avoring matters, prepared` from the'l distillate the pH of which was not adjusted prior to ether extraction.

This anhydrous ether extract, which does not contain Vvolatile acids,`may be used in any desired manner, either to adjust the avor'relation of the ultimate dry concen- V trate with the tiavorvalues of theaqueous extraction of -thecotee, or to f ortify any aqueous extraction where desired, or'may Abe satisfactorily carried over through` periods vof necessary shutdown of the process to restore the vvolatile flavoring matters which might otherwise be lost.

V`Theanhy`drous ether. extract prepared from the neutralized distillate' is 'also a separately usable productand "may be incorporated in any dry coffee concentrate to restore fullavorin'g matterthe'reto.

' The pIfI valueof the coiee brew is particularly related yto the judgment ofavorvalue ofthe entire brew and iltrhasbee'n'foundthat a small variation in pH of the "coffee brew"will result yin avery pronounced change in judgment ofV the avoring values of the brew. Thus Where, as in the process of Figure 2, the acid values of the ycoffee have been reduced, I have found that in order to meet such change in flavor judgment as may be influenced by the change of the pH value, that it is desirable to restore the acid removed. This may be done in any suitable manner as, for example, illustrated in the diagrammatic flow sheet of the process shown in Figure 3 by the incorporation o-f a suitable acid to the aqueous extract prior to vacuum concentration thereof. A suitable acid for such use is citric acid, ascorbic acid, or a volatile acid such as acetic acid may be incorporated in the aqueous extraction after vacuum evaporation to raise a solid content, this being to avoid loss of the acetic acid as far as-possible through volatilization during the concentration. It may be preferable where ascorbic acid is used to incorporate this acid in the dry coffee concentrate prior to mixing with the anhydrous ether extract.

I prefer to reincorporate the desired acid in the aqueous extract as above set forth rather than in the anhydrous ether extract because to add the acid to the anhydrous ether extract would increase its rate of deterioration. In this manner I have -found it desirable -to add such acid as may be required to the aqueous extract so that the resulting brew produced upon addition of water to the dry coffee concentrate will have a pH value of approximately 5, depending somewhat upon the coffee originally utilized in the process.

In Figure 4 I have shown a further modification of the process embodying my invention which reincorporates volatile fiavoring matters in the dry coffee concentrate powder produced in such manner as to produce dry coffee concentrate having the greatest avor maintaining characteristics. In this process the essential difference is that the anhydrous substantially acid free ether extract is distilled to remove the ether leaving a liquid avor concentrate which is etherand water-free and which has the greatest flavor retention values. This flavor concentrate which is etherand water-free is added to the concentrated aqueous extract. The solid content of this concentrated aqueous extract is preferably such that its solid content is between 25 and 60% by weight. It is found that it should be above 25% to exercise its retentive characteristic upon the fiavor values of the flavor concentrate. It should not be above 60% solids because of the required fluidity in order to obtain proper mixing of the avor concentrate with the body material.

The mixed concentrated aqueous extraction and flavor concentrate are then spray dried, producing a coffee concentrate with restored avoring having the desired adjusted pH and in which the volatile avorings are so reincorporated with the body material as to produce a coffee concentrate powder which has long-lasting full flavor characteristics.

It will be obvious from the foregoing that the particular conditions of operation selected for. use are those which meet the precise conditions desired. The greatest results are obviously obtained by following the process as diagrammatically illustrated in Figure 4. However, a satisfactory product may be produced in accordance with particular conditions without carrying the process to the extremity of the Figure 4 process.

I have herein set forth the best known method of carrying out my invention and my invention is defined in the appended claims.

I claim:

l. A process of preparing a dry coffee concentrate with restored volatile flavoring constituents, including the steps of introducing steam into the ground roasted coffee to wet and to liberate the volatile constituents thereof, condensing the steam and volatiles mixture to form an extract of the volatile constituents of the coffee, neutralizing the extract of the volatile constituents of the coffee, extracting the volatile constituents of the coffee with a solvent to remove the water therefrom, subsequently treating the ground vroasted coffee with water to form an aqueous ex- 6 traction, concentrating the aqueous extraction to reduce the water content thereof, drying the concentrated aqueous extraction and then mixing the solvent extraction with the dry aqueous extraction, and then removing the sol vent from the mixture.

2. A process of preparing a coffee concentrate, including the steps of wetting the ground coffee and then extracting the volatile constituents of the coffee to form a small volume of water extract containing said volatile constituents, neutralizing the water extract, separating the water from the neutral volatile constituents with a solvent, passing water through ground coffee to prepare a water extract therefrom, concentrating the latter extract by volatilizing water therefrom, mixing the solvent extract of volatile constituents with the concentrate of the latter extract, and then concentrating the mixture.

3. A process of preparing a full avored coffee concentrate comprising: obtaining a steam distillate of the volatile fiavo'ring matters separating the body materials with hot water to form an aqueous extract, neutralizing the steam distillate to a pH value of between 6 and 7, extracting avor matters from the neutralized steam distillate with ethyl ether, dehydrating the ether extraction, removing the ether from the ether extraction to leave a water-free avor concentrate, concentrating the aqueous extraction to where the samecontains 25 to 60% solids, mixing the concentrated aqueous extraction with the avor concentrate, and drying the mixture.

4. A process of preparing a full avored coffee concentrate comprising: obtaining a steam distillate of the volatile fiavoring matters, separating the body materials with hot water to form an aqueous extract, adjusting the pH of the aqueous extract by adding an edible acid thereto, neutralizing the steam distillate to a pH value of between 6 and 7, extracting flavor matters from the neutralized steam distillate with ethyl ether, dehydrating the ether extraction, removing the ether from the ether extraction to leave a water-free flavor concentrate, concentrating the aqueous extraction to where the same contains 25 to 60% solids, mixing the concentrated aqueous extraction with the flavor concentrate, and drying the mixture.

.5. A process of preparing a full fiavoredv coffee concentrate comprising: obtaining a steam distillate of the volatile ffavoring matters, separating the body materials with hot water to form an aqueous extract, neutralizing the steam distillate to a pH value of between 6 and 7, adding salt to the neutralized steam distillate to aid in the separation of the avor constituents from the neutralized steam distillate by extracting avor matters from the neutralized steam distillate with ethyl ether, dehydrating the ether extraction, removing the ether from the ether extraction to leave a water-free flavor concentrate, concentrating the aqueous extraction to where the same contains 25 to 60% solids, mixing the concentrated aqueous extraction with the avor concentrate, and drying the mixture.

6. In the process of preparing a full avored dry coffee concentrate, the steps of separating the volatile avoring constituents by steam distillate of wet ground coffee, separating an aqueous extraction of the body material of the coffee, neutralizing the steam distillate to a pH value of between 6 and 7, separating the volatile avoring matters from the steam distillate with a solvent such as ethyl ether, dehydrating the ether extr-action with an anhydrous salt and separating the salt therefrom by filtration, distilling off the ethyl ether to provide a avor concentrate which is water-free, concentrating the aqueous extraction, mixing the concentration of the aqueous extration with the avor concentrate, and drying the mixture.

7. In the process of preparing a full favored dry coffee concentrate, the steps of separating the volatile flavoring constituents by steam distillate of Wet ground coffee, separating an aqueous extraction of the body material of coffee, neutralizing the steam distillate to a pH value of between 6 and 7, separating the volatile avoring matters Afrom the steam distillatewith addedsalt to make a brine and using a solvent such asethyl ether, dehydrating the ether 'extraction with ananhy'drous saltandl separating the salt 4therefrom by filtration, distilling ol the ethyl *ether to provide a flavor concentrate which is water-tree, concentrating the aqueous extraction, mixing the concentration of the aqueous extraction rwith the flavor concentrate, drying the mixture, and adding lan edible acid to the aqueous extraction prior' tol mixingwith the avor concentrate to adjust the pH Value of a brew prepared from the'dry'coffce concentrate when mixed'with Water to a pH value of approximately 5.

8. A process of preparing'acoee avor concentrate including the steps'of introducingsteam into the ground roasted'colee to wet and to liberate the volatile constituents' thereof, condensing the steam and volatiles mixyture-to form Van extract of the volatile constituents of the coffee, neutralizing the extract of the volatile constituents 9. YA process -ot/'preparing aY coffee avor concentrate kfrom ground coiee comprisingz-obtaining a stearnudistillate of the volatile -avoring vmatters from the` ground coffee; neutralizing theV steam distillate to afpH value of between 6 and 7, extracting'flavor=-matters from-the neutralized' steam distillate with ethyl ether,l dehydrating the ether extraction, and removing-the etherfromthe ether extraction t-o leave a water-free avor concentrate.

VReferences Cited in the file of this Vpatent UNITED STATESA PATENTS j 439,318 einem; 1 o'ct. 2s, 1890 r'1,123,827 *Whitaker-et al. '.lan. 5,"1915 -1,123,828 j-uxfl'litaker` et al. Ian. 5K,` '|1915 1,251,359 MEtix DeCJZS, 1917 1,367,716 yPrattret* al; Feb. 8,1?1921 2,098,961 Fronrnuller Nov; 16,"1937 2,345,378 VVBrandt Mar. 28,11944 20 2,562,206 UNutting" "Iuly 31, 1951 FoREiGN PATENTS 2,013 Great IBritain 1913 289 Australia *July 13,l 1926 

1. A PROCESS OF PREPARING A DRY COFFEE CONCENTATTE WITH RESTORED VOLATILE FLAVORING CONSTITUENTS, INCLUDING THE STEPS OF INTRODUCING STEAM INTO THE GROUND ROASTED COFFEE TO WET AND TO LIBERATE THE VOLATILE CONSISTUENTS THEREOF, CONDENSING THE STEAN AND VOLATILES MIXTURE TO FORM AN EXTRACT OF THE VOLATILE CONSISTUENTS OF THE COFFEE, NEUTRALIZING THE EXTRACT OF THE VOLATILE CONSISTUENTS OF THE COFFEE, EXTRACTING THE VOLATILE CONSISTUENTS OF THE COFFEE WITH A SOLVENT TO REMOVE THE WATER THEREFROM, SUBSEQUENTLY TREATING THE GROUND ROASTED COFFEE WITH WATER TO FORM AN AQUEOUS EXTRACTION, CONCENTRATING THE AQUEOUS EXTRACTION TO REDUCE THE WATER CONTENT THEREOF, DRYING TEH CONCENTRATED AQUEOUS EXTRACTION AND THEN MIXING THE SOLVENT EXTRACTION WITH THE DRY AQUEOUS EXTRACTION, AND THEN REMOVING THE SOLVENT FROM THE MIXTURE. 